CN206848304U - The hot many reference amounts coupling microscope probe of magnetoelectricity - Google Patents

Abstract

The utility model provides a magnetic-electric-thermal multi-parameter coupling microscope probe, which includes a probe arm and a needle tip body connected to the probe arm, and from the surface of the probe arm and the needle tip body to the outside, the thermocouples are sequentially covered layer, thermally conductive insulating layer and magnetic conductive layer; thermocouple layer and external circuit form a thermoelectric circuit; magnetic conductive layer forms a conductive circuit with sample and external circuit. The probe has a simple structure and low preparation difficulty, can detect the magnetic signal, electrical signal and thermal signal of the magnetoelectric functional material in situ, and can effectively avoid the signal interference between the thermoelectric circuit and the electric circuit.

Description

Magnetic-electrical-thermal multi-parameter coupled microscope probe

technical field

The utility model relates to a probe of a scanning probe microscope, in particular to a magnetic-electric-thermal multi-parameter coupled microscope probe.

Background technique

With the rapid development of information technology, the electronic components of integrated circuits tend to be miniaturized and integrated. The size of electronic components has entered the micro/nano scale, and its heat generation and heat dissipation problems have become bottlenecks restricting further high integration. Characterizing heat-related physical properties at the micro/nano scale and understanding the physical processes of heat generation and heat dissipation have become a new branch of modern thermal science—micro/nano-scale thermal science. At the micro/nano scale, the microstructure and domain structure (for magnetic and ferroelectric materials) of materials have a particularly important influence on thermal properties. A microcrack, hole, grain boundary, or even a domain wall may affect the thermal properties of the material. thermal properties. Taking multiferroic materials as an example, magnetic/electrical domain flipping (or domain wall movement) and leakage current driven by an external field will both cause micro-region heating. Although people have developed a variety of technical means to study these parameters, so far, there is no technology and equipment that can perform in-situ-real-time-synchronous comprehensive characterization of these parameters, which limits the in-depth understanding of the physical mechanism of heat generation and heat dissipation in materials. Therefore, it is impossible to find a solution to the problem of heat generation and heat dissipation of materials at the micro/nano scale.

As an important research method of nano science and technology, atomic force microscope technology has been developed rapidly. Scanning probe microscope technology is developed on the basis of scanning tunneling microscope. It has many advantages such as high spatial resolution, variable temperature work in vacuum, atmosphere, and even solution, etc., which makes it widely used in Physics, chemistry, biology, electronics and other research fields. People detect the surface morphology and other physical properties of the sample by detecting physical quantities such as various interaction forces or currents between the probe and the sample surface, and develop technologies such as atomic force microscope, magnetic force microscope, piezoelectric force microscope, and conductive force microscope. , can be used to detect physical parameters such as sample surface morphology, domain structure, micro-region conductance, etc.

In recent years, the scanning thermal probe technology has been newly developed, and the scanning probe microscopy technology has been expanded to the field of thermal research, and the spatial distribution characterization and research of thermal properties such as temperature and thermal conductivity of the surface micro-regions of materials and devices have been realized. Although people have developed micro-area thermal imaging technology based on scanning probe microscopy, at present, based on this technology, only thermal information can be obtained alone, and it is not possible to simultaneously obtain magnetic domain structure and ferroelectric/piezoelectric domain structure simultaneously in situ and in real time. , conductive domain structure and many other information, especially the correlation between the period is not clear, and magnetic-electric-thermal coupling imaging cannot be performed, which limits the in-depth understanding of the physical mechanism of heat generation and heat dissipation in materials, so that it is impossible to find out the solution of the material. Heat generation and heat dissipation at the micro/nano scale.

The utility model proposes a novel nanometer magnetic-electrical-thermal multi-parameter coupling microscope probe, which will overcome the limitations of the existing single magnetic, electric and thermal functional modules, and develop a probe with magnetic-electrical-thermal characteristic detection , equipped with a corresponding signal detection and processing system, will be able to realize the in-situ characterization of changes in magnetic domains, ferroelectric domains, micro-domain conductance, and micro-domain heating properties and their correlations. Therefore, in the field of nano-testing technology, the development of new nano-characterization technology, especially probe characterization technology is one of the research hotspots in related research fields.

Utility model content

Aiming at the above-mentioned technical status, the utility model provides a nano-magnetic-electric-thermal multi-parameter coupling microscope probe, which has a simple structure and can measure multiple physical parameters such as magnetism, electricity and heat in situ and synchronously, and realize magnetic domain, electric Research on the influence of domains on thermal properties.

The technical solution of the utility model is: a magnetic-electric-thermal multi-parameter coupling microscope probe, including a probe arm, and a needle tip body connected to the probe arm, the tip of the needle tip body is used to contact the sample or not Contact to measure the signal of the sample; its feature is: from the surface of the needle tip body to the outside, there are thermocouple layer, thermal insulating layer, and magnetic conductive layer in sequence;

The thermocouple layer covers the area A and area B on the surface of the needle tip body, the area on the surface of the needle tip body except area A and area B is the remaining area, and there is no overlapping area between area A and area B and it is at the tip of the needle point body Connected; the material covering area A is material A, the material covering area B is material B, material A is different from material B, and forms a thermoelectric circuit with an external circuit;

The thermally conductive insulating layer covers the remaining area of the thermocouple layer and the surface of the tip body;

The magnetic conductive layer is located on the surface of the thermally conductive insulating layer, at least covers the tip of the needle point body, and forms a conductive loop with the sample and the external circuit.

The three-dimensional structure of the needle tip body is not limited, and may be a pyramid, a cone, a prism, a truncated cone, and the like.

In order to improve detection sensitivity, preferably, the region A and region B are not connected except for the tip of the needle tip.

Preferably, the probe arm surface includes area A' and area B', area A' and area B' have no overlapping area, area A' is connected with area A, area B' is connected with area B; the external circuit It includes material A covering the surface of area A', and material B covering the surface of area B'.

The material A and material B are electrically conductive, and they are connected to form a circuit. When the temperature of the connection point changes, a potential difference is generated in the thermocouple circuit. The material A is not limited, and includes one material or a combination of two or more materials in metals and semiconductors with good electrical conductivity, such as palladium, gold, bismuth (Bi), nickel (Ni), cobalt (Co), At least one of metals such as potassium (K) and alloys thereof, and semiconductors such as graphite and graphene. The material B is not limited, and includes one material or a combination of two or more materials in metals and semiconductors with good electrical conductivity, such as palladium, gold, bismuth (Bi), nickel (Ni), cobalt (Co), At least one of metals such as potassium (K) and alloys thereof, and semiconductors such as graphite and graphene.

The thermally conductive insulation has thermal conductivity and electrical insulation at the same time, and its material is not limited, including semiconductors, inorganic materials or organic materials with certain insulating properties, such as zinc oxide (ZnO), bismuth ferrite (BiFeO ₃ ), cobalt Lithium oxide (LiCoO ₂ ), nickel oxide (NiO), cobalt oxide (Co ₂ O ₃ ), copper oxide (Cux O), silicon dioxide (SiO ₂ ), silicon nitride (SiN _{x )} , titanium dioxide (TiO ₂ ), tantalum pentoxide (Ta ₂ O ₅ ), niobium pentoxide (Nb ₂ O ₅ ), tungsten oxide (WO _x ), hafnium dioxide (HfO ₂ ), aluminum oxide (Al ₂ O ₃ ), graphite oxide olefin, amorphous carbon, copper sulfide ( _CuxS ), silver sulfide (Ag ₂ S), amorphous silicon, titanium nitride (TiN), polyimide (PI), polyamide (PAI), polysieffer At least one of alkali (PA), polysulfone (PS) and the like.

The magnetic conductive layer has magnetism and conductivity, and its material is not limited, including ferromagnetic metals such as iron (Fe), cobalt (Co), nickel (Ni) and magnetic alloys.

In order to facilitate the connection of external circuits, the ferromagnetic conductive layer can also cover other parts of the needle point body except the tip part. As an implementation method, in the working state, the ferromagnetic conductive layer is in contact with the sample, the sample is grounded, and the external circuit is connected to the ferromagnetic conductive layer, that is, the external circuit, the ferromagnetic conductive layer, the sample and the earth constitute an electrical circuit for Measure the electrical signal of the sample.

The utility model also provides a method for preparing the above-mentioned magneto-electric-thermal multi-parameter coupled microscope probe, comprising the following steps:

Step 1: Using magnetron sputtering technology to deposit material A on the surface of area A of the tip body, and deposit material B on the surface of area B to obtain a thermocouple layer;

Step 2: using magnetron sputtering technology or pulsed laser technology to deposit a thermally conductive insulating layer on the surface of the thermocouple layer and the rest of the surface of the tip body except for region A and region B;

Step 3: Depositing a magnetic conductive layer on the surface of the thermally conductive insulating layer by using magnetron sputtering technology.

Utilize the magnetic-electric-thermal multi-parameter coupling microscope probe of the present utility model to detect the morphology, magnetic signal, electrical signal and thermal signal of the sample, and its detection method is as follows:

(1) Surface morphology and magnetic signal detection of samples

Use contact mode.

That is, the probe driving unit drives the probe so that the tip of the needle tip body is displaced to an initial position on the sample surface, and the probe performs directional scanning on the sample surface from the initial position, and the point contact between the tip of the needle tip body and the sample surface is controlled during the scanning process Or vibration point contact, collect the displacement signal or vibration signal of the needle tip body, and obtain the shape signal of the sample after analysis;

The probe returns to the initial position and lifts up a certain distance, and then scans the sample surface according to the orientation. During the scanning process, the tip of the needle tip body is controlled to move or vibrate along the topography image, and the needle tip is collected. The displacement signal or vibration signal of the body is analyzed to obtain the magnetic signal image of the sample.

(2) Thermal signal detection of samples

The external circuit and the thermocouple layer of the probe form a closed thermoelectric loop, and when the temperature of the connection point changes, the potential difference changes in the thermocouple loop. When the tip of the tip body is in contact with the surface of the sample, the tip body exchanges heat with the sample through the covering layers of the tip, so that the potential difference in the thermal circuit changes, and the thermal signal image of the sample is obtained after collection and analysis.

(3) Electrical signal detection of samples

The tip of the tip body is in contact with the sample surface, and the external circuit, the magnetic conductive layer of the probe, and the sample form a closed electrical circuit, that is, the electrical signal flows into the magnetic conductive layer of the probe and the sample to form a voltage signal, which is collected and analyzed , to obtain the electrical signal image of the sample.

Compared with the prior art, the utility model adopts a thermocouple structure, the thermocouple layer and the external power supply independently form a thermoelectric circuit, the sample to be tested, the magnetic conductive layer and the external power supply independently form an electric circuit, and the thermally conductive insulating layer is located between the thermal resistance layer and the external power supply. Between the magnetic conductive layers, the signal interference between the thermoelectric circuit and the electric circuit is effectively blocked, and the magnetic signal, electrical signal and thermal signal of the magnetoelectric functional material can be detected in situ, including the magnetic field at the micron and nanometer scales. In situ microprobing of signal, electrical and thermal signals.

Description of drawings

Fig. 1 is a schematic view of the front structure of the probe arm and the tip body of the magnetic-electric-thermal multi-parameter coupled microscope probe in Example 1 of the present invention;

Fig. 2 is a schematic diagram of the side structure of Fig. 1;

Fig. 3 is an enlarged schematic diagram of the thermocouple layer on the surface of the tip body shown in Fig. 1;

Fig. 4 is the structural representation of thermocouple layer and part external circuit shown in Fig. 3;

Fig. 5 is a schematic structural view of the surface of the probe shown in Fig. 4 covered with a thermally conductive insulating layer;

6 and 7 are structural schematic diagrams of the surface of the probe shown in FIG. 5 covered with a magnetic conductive layer.

Among them: 1 probe arm, 2 needle point body, 3 one side of the needle point body, 4 the other side of the needle point body, 5 the front of the needle point body, 6 the back of the needle point body, 7 thermal insulation layer, 8 magnetic conductive layer.

detailed description

The utility model will be further described in detail below in conjunction with the examples. It should be pointed out that the following examples are intended to facilitate the understanding of the utility model, and do not limit the utility model in any way.

Example 1:

In this embodiment, a commercially available uncoated Si probe is selected, and its structure is shown in FIG. 1 , including a probe arm 1 and a tip body 2 connected to the probe arm 1 . As shown in FIGS. 1 and 2 , the needle point body 2 has a tetrahedral pyramid structure, and is composed of a front surface 5 , a back surface 6 opposite to the front surface, and two side surfaces 3 and 4 .

As shown in FIG. 3 , the surface of the needle tip body is divided into a region A and a region B, and regions other than the region A and region B are the remaining regions. The area filled with lines in the surface of the needle point body in Figure 3 is area A (that is, one side 3 of the needle point body), the area filled with rectangles is area B (that is, the other side 4 of the needle point body), and area A and area B There are no overlapping areas and are connected only at the tip of the tip body.

As shown in Figure 4, the surface of the probe arm includes area A' and area B'. In Figure 4, the area filled with lines on the surface of the probe arm is A', the area filled with rectangles is B', and there is no area A' and area B'. Regions overlap and are not connected, region A' is connected to region A, and region B' is connected to region B.

The following covering layer was prepared on the surface of the probe.

(1) Clean the uncoated Si probe with 50000 Hz ultrasonic wave for 5 min.

(2) As shown in Figure 3, design a mask plate of a specific shape and size, use magnetron sputtering technology or pulsed laser technology, evaporate platinum on the surface of area A, and evaporate gold on the surface of area B to form a thermocouple Floor. Then, as shown in Fig. 4, platinum is vapor-deposited on the surface of the region A', and gold is vapor-deposited on the surface of the region B' to constitute a part of the external circuit. The thermocouple layer and the external circuit constitute a thermoelectric circuit for measuring the thermal signal of the sample.

(3) As shown in Figure 5, using magnetron sputtering technology or pulsed laser technology on the surface of the thermocouple layer, and the remaining areas of the surface of the tip body except for area A and area B (that is, the front surface of the tip body 5 Deposit silicon dioxide on the surface of the back side 6) to obtain a thermally conductive insulating layer 7, as shown in the horizontal line filling in Figure 5;

(4) As shown in FIG. 6 , use magnetron sputtering technology or pulsed laser technology to deposit an iron-based magnetic conductive layer 8 on the surface of the thermally conductive insulating layer on the surface of the thermocouple layer, as shown in FIG. 6 filled with grid lines. The ferromagnetic conductive layer is connected to the external circuit. In the working state, the ferromagnetic conductive layer is in contact with the sample, the sample is grounded, and the external circuit is connected to the ferromagnetic conductive layer. That is, the external circuit, the ferromagnetic conductive layer, the sample and the earth constitute an electric circuit. Loop for measuring the electrical signal of the sample.

When using the above-mentioned probe to detect the morphology and magnetic signal, thermal signal and electrical signal of the sample, the detection method is as follows:

(1) Used to detect the surface morphology and magnetic signal of the sample

The probe driving unit drives the probe so that the tip of the tip body moves to an initial position on the sample surface, and the probe scans the sample surface in a transverse direction from the initial position, and controls the point contact between the tip of the tip body and the sample surface during the scanning process Or vibration point contact, collect the longitudinal displacement signal or vibration signal of the needle tip body, and obtain the shape signal of the sample after analysis;

The probe returns to the initial position and lifts up a certain distance, and then scans the surface of the sample according to the lateral orientation, and controls the tip of the needle body to move longitudinally or vibrate along the topography image during the scanning process, The longitudinal displacement signal or vibration signal of the needle tip body is collected, and the magnetic signal image of the sample is obtained after analysis;

(2) Used to detect the thermal signal of the sample

The external circuit and the thermocouple layer of the probe form a closed thermal circuit. When the temperature of the connection point at the tip of the needle tip changes, the potential difference changes in the thermocouple circuit; the probe driving unit drives the probe to move to a certain position on the sample surface, so that the tip body The tip is in contact with the surface of the sample, and the body of the needle tip exchanges heat with the sample through each covering layer, so that the potential signal in the thermal circuit changes, and the thermal signal image of the sample is obtained after collection and analysis;

(3) Electrical signals used to detect samples

The probe driving unit drives the probe to move to a certain position on the sample surface, so that the tip of the tip body contacts the sample surface, and the external circuit, the magnetic conductive layer of the probe, and the sample form a closed electrical circuit, that is, the electrical signal flows into the probe The magnetic conductive layer and the sample form a voltage signal, which is collected and analyzed to obtain the electrical signal image of the sample.

Example 2:

In the present embodiment, the probe structure is basically the same as the Si probe structure in Example 1, the only difference being that the described step (4) is as follows:

As shown in FIG. 7 , magnetron sputtering technology or pulsed laser technology is used to deposit an iron-based magnetic conductive layer 8 on the surface of the thermocouple layer and on the surface of the heat-conducting insulating layer, as shown in the grid line filling in FIG. 7 . That is, compared with FIG. 6 , the iron-based magnetic conductive layer 8 in FIG. 7 covers the entire front surface of the probe tip and the front end of the probe body. This structure facilitates the connection of the magnetic conductive layer to external circuits. In the working state, the ferromagnetic conductive layer is in contact with the sample, the sample is grounded, and the external circuit is connected to the ferromagnetic conductive layer, that is, the external circuit, the ferromagnetic conductive layer, the sample and the earth form an electrical circuit for measuring the electrical signal of the sample. .

The above-described embodiments have described the technical solutions of the utility model in detail. It should be understood that the above descriptions are only specific embodiments of the utility model, and are not intended to limit the utility model. Any amendments, supplements or substitutions made in similar ways, etc., shall be included in the protection scope of the present utility model.

Claims (4)

1. a kind of magnetic-electric-thermal many reference amounts coupling microscope probe, including feeler arm, and the needle point body being connected with feeler arm, The tip of the needle point body is used to contact with sample or non-contact, to measure sample signal；It is characterized in that：From needle point body Surface is outside, is followed successively by thermoelectricity double-layer, thermally conductive insulating layer, magnetic conductive layer；

Described thermoelectricity double-layer is covered with the region A and region B of needle point body surface, and needle point body surface is except region A and area Region outside the B of domain is remaining area, region A regions non-overlapping with region B and is connected at the sophisticated position of needle point body； Overlay area A materials A, and the overlay area B material Bs different from materials A, electrothermal circuit is formed with external circuit；

Described thermally conductive insulating layer is covered with the remaining area of thermoelectricity double-layer and needle point body surface；

Described magnetic conductive layer is located at heat conductive insulating layer surface, is at least covered with the sophisticated position of needle point body, with sample, outside Portion's circuit forms galvanic circle.

2. magnetic according to claim 1-electric-thermal many reference amounts coupling microscope probe, it is characterized in that：Described needle point body Three-dimensional structure include pyramid, circular cone, terrace with edge, round platform.

3. magnetic according to claim 1-electric-thermal many reference amounts coupling microscope probe, it is characterized in that：Described region A with Region B is not connected with addition to the position of needle point tip.

4. magnetic according to claim 1-electric-thermal many reference amounts coupling microscope probe, it is characterized in that：Feeler arm surface includes Region A ' and the non-overlapping region of region B ', region A ' and region B ', region A ' are connected with region A, and region B ' is connected with region B Connect；Described external circuit includes being covered with the materials A on region A ' surfaces, and is covered with the material B on region B ' surfaces.